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One-step method for preparing neonicotinoid pesticide core-shell mesoporous surface molecularly imprinted polymer

A surface molecular imprinting, neonicotinoid technology, applied in chemical instruments and methods, preparation of test samples, other chemical processes, etc., can solve problems such as unfavorable rapid detection, long preparation time of molecularly imprinted polymers, etc. Blotting time, increasing adsorption capacity and mass transfer rate, effect of increasing adsorption capacity

Active Publication Date: 2021-02-19
UNIV OF SHANGHAI FOR SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is: the preparation time of molecularly imprinted polymer is long at present, which is not conducive to the problem of rapid detection

Method used

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  • One-step method for preparing neonicotinoid pesticide core-shell mesoporous surface molecularly imprinted polymer
  • One-step method for preparing neonicotinoid pesticide core-shell mesoporous surface molecularly imprinted polymer

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preparation example Construction

[0028] Wherein: the preparation method of nano-silica microspheres described in step S1 includes: adding absolute ethanol and ultrapure water to the reaction vessel, then adding ammonia water with a mass concentration of 25%, stirring magnetically at 500-800rpm for 5-10min, and then Add tetraethoxysilane, continue magnetic stirring, and centrifuge to collect the product after the reaction, and dry it in a vacuum oven at 60°C overnight to obtain silica microspheres; add porogens such as CTAB or P123 to the preparation, and Mesoporous silica microspheres can be obtained by elution.

[0029] The modification of the vinyl functionalization in step S2 includes: adding the prepared silica microspheres and toluene into the reaction vessel, and adding 3-(methacryloyloxy)propyltrimethoxysilane after they are mixed uniformly, and then Stir in an oil bath at 90°C for 24-36 hours. After the reaction, the product is collected by centrifugation and dried overnight in a vacuum oven at 60°C. ...

Embodiment 1

[0032] The one-step method for preparing neonicotinoid pesticide core-shell mesoporous surface molecularly imprinted polymers includes the following steps:

[0033] S1: Add 40mL ultrapure water to the round bottom flask, then add 10mL ethanol and ammonia water, stir magnetically at 500rpm for 10min, then add 10mL tetraethyl orthosilicate, continue magnetic stirring, centrifuge to collect samples after the reaction, and store at 60°C Drying under low temperature can obtain nano-silica microspheres;

[0034] S2: Take 0.5g of nano-silica microspheres prepared in S1 in the reaction vessel, then add 100mL of toluene, after stirring evenly, add 2mL of 3-(methacryloyloxy)propyltrimethoxysilane , stirred in an oil bath at 90°C for 36 hours, centrifuged to collect the product after the reaction, and dried overnight in a vacuum oven at 60°C;

[0035] S3: Add 0.14 mmol of imidacloprid to the reaction vessel, then add 0.72 mmol of methacrylic acid and 100 mL of acetonitrile, stir for 1 h...

Embodiment 2

[0044] The one-step method for preparing neonicotinoid pesticide core-shell mesoporous surface molecularly imprinted polymers includes the following steps:

[0045] S1: Add 50mL ultrapure water to the round bottom flask, then add 10mL ethanol and ammonia water, stir magnetically at 500rpm for 10min, then add 14mL tetraethyl orthosilicate, continue magnetic stirring, centrifuge to collect samples after the reaction, and store at 60°C Drying under low temperature can obtain nano-silica microspheres;

[0046] S2: Take 0.5g of nano-silica microspheres prepared in S1 in the reaction vessel, then add 100mL of toluene, after stirring evenly, add 2mL of 3-(methacryloyloxy)propyltrimethoxysilane , stirred in an oil bath at 90°C for 36 hours, centrifuged to collect the product after the reaction, and dried overnight in a vacuum oven at 60°C;

[0047] S3: Add 0.14 mmol of imidacloprid to the reaction vessel, then add 0.72 mmol of acrylamide and 100 mL of acetonitrile, stir for 1 h, weig...

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Abstract

The invention discloses a method for preparing a neonicotinoid pesticide core-shell mesoporous surface molecularly imprinted polymer by a one-step method, which is characterized by comprising the following steps: preparing silicon dioxide microspheres; carrying out vinyl functionalized modification on the silicon dioxide microspheres; mixing and stirring a template molecule neonicotinoid pesticideand a functional monomer in acetonitrile for prepolymerization, adding hexadecyltrimethylammonium bromide in the synthesis process of the molecularly imprinted polymer, adding an initiator, a cross-linking agent and a silanization reagent, and removing hexadecyltrimethylammonium bromide and the template molecule neonicotinoid pesticide to obtain the core-shell mesoporous surface molecularly imprinted polymer. The core-shell mesoporous surface molecularly imprinted polymer capable of specifically recognizing and adsorbing the neonicotinoid pesticide is prepared through a one-step method, on one hand, mesopores are beneficial to transmission of a template and combination of inner-layer imprinting sites, and the imprinting effect and the mass transfer rate are increased; and on the other hand, the preparation time of the imprinted polymer can be shortened, the requirement of rapid detection is met, and the imprinted polymer is used for rapid detection.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional materials, and in particular relates to a method for preparing neonicotinoid pesticide core-shell mesoporous surface molecularly imprinted polymers in one step. Background technique [0002] Neonicotinoid pesticides are widely used in agriculture to control insects and seeds on crops, and their residues may exist in fruits, vegetables, soil and grains, and they have a strong affinity for acetylcholinesterase receptors. The characteristics of neonicotinoid pesticides will cause certain toxicity to the liver and kidney, so even low residual neonicotinoid pesticides will have adverse effects on human health and safety. [0003] At present, the methods commonly used to detect neonicotinoid pesticides include: gas chromatography tandem mass spectrometry (GC-MS), liquid chromatography tandem mass spectrometry (LC-MS), optical methods, electrochemical methods, etc. Although these metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08F220/06C08F222/14C08J9/28C08J9/26B01J20/26B01J20/30G01N1/28C08L51/10
CPCC08F292/00C08J9/28C08J9/26B01J20/264G01N1/28C08J2351/10C08F220/06C08F222/102
Inventor 阴凤琴霍凯旋徐斐袁敏曹慧叶泰吴秀秀
Owner UNIV OF SHANGHAI FOR SCI & TECH
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